Experiment Report of Laboratory

Organization

Preparation of NH4OH 2M 25% Solution

Arranged by Group 6:

1. Astri Nurul H (113194016)

2. Ciko Rolly (1131940xx)

3. Fibri Erwan S (1131940xx)

4. Nurul Aina Putri (1131940xx)

5. Siti Masrifah (113194034)

6. Aura (xxxxxxxxx)

International Chemistry Education

STATE UNIVERSITY OF SURABAYA

MATHEMATIC AND NATURAL SCIENCE FACULTY

CHEMISTRY DEPARTMENT

2014

I. TITLE : Preparation of NH4OH 2M 25% Solution

II. DATE : Monday, February 24th 2014

III. OBJECTIVE : To prepare 250 mL NH4OH 2M 25% solution

IV. BASIC THEORY :

A. Material Safety Data Sheet (MSDS) of NH3

DESCRIPTION

CHEMICAL NAME : Ammonia, Anhydrous

SYNONYMS : Ammonia

FORMULA : NH3

CHEMICAL FAMILY : Inorganic

MOL. WT. : 17.03(NH3)

COMPOSITION : 99+% Ammonia

STATEMENT OF HEALTH HAZARD

HAZARD DESCRIPTION: Ammonia is an irritant and corrosive to the skin,

eyes, respiratory tract and mucous membranes. May cause severe burns to the

eyes, lungs and skin. Skin and respiratory related diseases could be aggravated by

exposure

EMERGENCY TREATMENT

EFFECTS OF OVEREXPOSURE:

Eye: lacrimation, edema, or blindness may occur.

Skin: irritation, corrosive burns, blister formation may result. Contact with liquid

will freeze the tissue and produce a caustic burn.

Inhalation: acute exposure may result in severe irritation of the respiratory tract,

bronchospasm, edema or respiratory arrest.

Ingestion: Symptoms similar to Inhalation. Lung irritation and pulmonary edema

may occur.

Extreme exposure may result in death from spasm, inflammation or edema.

EMERGENCY AID:

Eye: flush with copious amounts of water for 15 minutes. Eyelids should be held

apart and away from eyeball for thorough rinsing.

Skin: flush with copious amounts of water for 15 minutes while removing

contaminated clothing and shoes. Exercise caution when removing contaminated

clothing as it may be frozen to the skin. Do not rub or apply ointment on affected

area.

Inhalation: remove to fresh air. Administer oxygen or artificial respiration if

necessary.

Ingestion: if conscious, give large amounts of water to drink or may drink orange

juice or citrus to counteract ammonia.

Do NOT induce vomiting.

NOTE TO PHYSICIAN: Lung injury and pulmonary edema may appear as a

delayed phenomenon. Supportive treatment with necessary ventilation actions,

including oxygen, may warrant consideration.

PHYSICAL DATA

BOILING PT: -33°C (-28°F)

FREEZING PT: -78ºC (-108°F)

VAPOR PRESSURE: 10 atm @ 25.7ºC

SOLUBILTY IN WATER: 89.9 g/100cc @ 0ºC 7.4 g/100cc @100ºC

SPECIFIC GRAVITY (H2O=1): 0.682 @ 4°C (39°F)

EVAPORATION RATE (Water=1): Faster than water

PERCENT VOLATILE: 100%

SURFACE TENSION: 23.4 Dynes/cm @ 11.1ºC

APPEARANCE &ODOR: Colorless gas/liquid and pungent odor

VAPOR DENSITY (AIR=1): 0.596 @ 0°C (32°F)

FIRE AND EXPLOSION HAZARD

SPECIAL FIRE-FIGHTING PROCEDURES:

Must wear protective clothing and a positive pressure SCBA. Stop source if

possible. Cool fire exposed containers with water spray. Stay upwind and use

water spray to knock down vapor and dilute.

UNUSUAL FIRE AND EXPLOSION HAZARDS:

Outdoors, ammonia is not generally a fire hazard. Indoors, in confined areas,

ammonia may be a fire hazard, especially if oil and other combustible materials

are present. If relief valves are inoperative, heat-exposed storage containers may

become explosion hazards. Ammonia contact with chemicals such as mercury,

chlorine, iodine, bromine, silver oxide, or hypochlorites can form explosive

compounds. Special hazards with chlorine to form chloramine gas, also a primary

skin irritant and sensitizer. Combustion may form toxic nitrogen oxides.

CHEMICAL REACTIVITY

STABILITY: Stable at room temperature. Ammonia will react exothermically

with acids and water.

CONDITIONS TO AVOID:

Explosive or violent reactions can occur from mixing ammonia with halogens,

strong oxidizers, strong mineral acids, Nitric Acid, Fluorine, Nitrogen Oxide,

etc…

Sensitive explosive mixtures can form when mixed with air and hydrocarbons,

Ethanol and Silver Nitrate, Chlorine, etc….

Explosive products are formed by the reaction of ammonia with Silver Chloride,

Silver Oxide, Bromine, Iodine, Gold, Mercury, Tellurium Halides, etc….

Ammonia is incompatible or has hazardous reactions with Silver, Acetaldehyde,

Acrolein, Boron, Halogens, Perchlorate, Chloric Acid, Chloric Monoxide,

Chlorites, Nitrogen Tetroxide, Tin, Sulfur, etc….

Ammonia has a corrosive reaction with galvanized surfaces, copper, brass, bronze,

aluminum alloys, mercury, gold, and silver. This is a partial list of

incompatibilities.

HAZARDOUS DECOMPOSITION PRODUCTS: Hydrogen and nitrogen

gases above 450ºC (842ºF). Decomposition temperatures may be lowered by

contact with certain metals.

SPILL OR LEAK PROCEDURES

STEPS TO BE TAKEN: Wear protective clothing and respiratory protection, see

Protective Equipment. Stop source if possible. If exposure concerns are present,

stay upwind and use water spray downwind of leak source to absorb ammonia gas

and dilute. Contain diluted run-off from drains, sewers, water systems, etc…

CAUTION: ADDING WATER DIRECTLY TO LIQUID SPILLS WILL

INCREASE VOLATILIZATION OF AMMONIA, THUS INCREASING

POSSIBILITY OF EXPOSURE.

WASTE DISPOSAL: Listed as a hazardous substance under CWA (40 CFR

1164.40 CFR 117.3 Reportable Quantity 100 lbs. OR 45.4kg) Classified as a

hazardous waste under RCRA (40 CFR 261.32 Corrosive # D002). Comply with

all Federal, State and local regulations. Suitably diluted product may be applied to

agricultural land as fertilizer. Keep spill from entering streams, lakes or any water

systems.

SPECIAL PROTECTION AND PROCEDURES

RESPIRATORY PROTECTION: MSHA/NIOSH approved respiratory

protection that consists of a full face gas mask and canisters effective for

anhydrous ammonia that enable use for entry and escape in emergencies. Refer to

29 CFR 1910.134 for requirements and selection. A positive pressure SCBA is

required for entry into ammonia atmospheres at or above 300 ppm.

VENTILATION: Local exhaust sufficient to keep ammonia gas below

Permissible Exposure Limits.

PROTECTIVE EQUIPMENT: Splash-proof, chemical safety goggles, rubber

gloves and boots should be worn to prevent contact. Face shield can be worn over

the goggles as added protection. Respiratory protection and cotton work clothes

are recommended. Refer to 29 CFR 1910.132 to 1910.136 for requirements. A

positive pressure SCBA is required for entry into ammonia atmospheres at or

above 300 ppm.

SPECIAL PRECAUTIONS

STORAGE AND HANDLING: Store in a cool, well-ventilated area with

containers tightly closed. OSHA 29 CFR 1910.111 prescribes handling and

storage requirements for anhydrous ammonia as a hazardous material.

WORK-PLACE PROTECTIVE EQUIPMENT: Protective equipment should

be stored near, but outside of ammonia area. Water for first aid, such as an

eyewash station and safety shower, is to be kept available in the immediate

vicinity. See 29 CFR 1910.141 for workplace requirements.

DISPOSAL: Ammonia is listed as a hazardous substance under FWPCA. It is

classified as RCRA hazardous waste due to corrosivity, See WASTE DISPOSAL.

PERSONAL: Use protective equipment as needed. Do not wear contact lenses.

Avoid unnecessary exposure.

B. Material Safety Data Sheet (MSDS) of NH4OH

Section 1: Chemical Product and Company Identification

Product Name: Ammonium hydroxide

Synonym: Aqueous Ammonia; Strong Ammonia Solution; Stronger Ammonia

Water

Section 2: Composition

Composition:

Name % by Weight

Ammonia, anhydrous 27-31

Water 69-73

Section 3: Hazards Identification

Potential Acute Health Effects:

Very hazardous in case of skin contact (corrosive, irritant, permeator), of eye

contact (irritant), of ingestion, . Non-corrosive to the eyes. Non-corrosive for

lungs. Liquid or spray mist may produce tissue damage particularly on mucous

membranes of eyes, mouth and respiratory tract. Skin contact may produce burns.

Inhalation of the spray mist may produce severe irritation of respiratory tract,

characterized by coughing, choking, or shortness of breath. Severe over-exposure

can result in death. Inflammation of the eye is characterized by redness, watering,

and itching. Skin inflammation is characterized by itching, scaling, reddening, or,

occasionally, blistering.

Potential Chronic Health Effects:

CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS:

Mutagenic for bacteria and/or yeast. [Ammonia, anhydrous]. TERATOGENIC

EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Not available. The

substance is toxic to upper respiratory tract, skin, eyes. Repeated or prolonged

exposure to the substance can produce target organs damage. Repeated or

prolonged contact with spray mist may produce chronic eye irritation and severe

skin irritation. Repeated or prolonged exposure to spray mist may produce

respiratory tract irritation leading to frequent attacks of bronchial infection.

Repeated exposure to a highly toxic material may produce general deterioration of

health by an accumulation in one or many human organs.

Section 4: First Aid Measures

Eye Contact:

Check for and remove any contact lenses. Immediately flush eyes with running

water for at least 15 minutes, keeping eyelids open. Cold water may be used. Get

medical attention immediately. Finish by rinsing thoroughly with running water to

avoid a possible infection.

Skin Contact:

In case of contact, immediately flush skin with plenty of water for at least 15

minutes while removing contaminated clothing and shoes. Cover the irritated skin

with an emollient. Cold water may be used. Wash clothing before reuse.

Thoroughly clean shoes before reuse. Get medical attention immediately.

Serious Skin Contact:

Wash with a disinfectant soap and cover the contaminated skin with an anti-

bacterial cream. Seek immediate medical attention.

Inhalation:

If inhaled, remove to fresh air. If not breathing, give artificial respiration. If

breathing is difficult, give oxygen. Get medical attention immediately.

Serious Inhalation:

Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such

as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the

victim is not breathing, perform mouth-to-mouth resuscitation. WARNING: It

may be hazardous to the person providing aid to give mouth-to-mouth

resuscitation when the inhaled material is toxic, infectious or corrosive. Seek

medical attention.

Ingestion:

If swallowed, do not induce vomiting unless directed to do so by medical

personnel. Never give anything by mouth to an unconscious person. Loosen tight

clothing such as a collar, tie, belt or waistband. Get medical attention

immediately.

Section 5: Fire and Explosion Data

Flammability of the Product: Non-flammable.

Products of Combustion:

Hazardous decomposition include Nitric oxide, and ammonia fumes

Explosion Hazards in Presence of Various Substances:

Non-explosive in presence of open flames and sparks, of shocks.

Special Remarks on Explosion Hazards:

Forms explosive compounds with many heavy metals such as silver, lead, zinc

and their halide salts. It can form shock sensitive compounds with halogens,

mercury oxide, and siliver oxide.

Section 6: Accidental Release Measures

Small Spill:

Dilute with water and mop up, or absorb with an inert dry material and place in an

appropriate waste disposal container. If necessary: Neutralize the residue with a

dilute solution of acetic acid.

Large Spill:

Corrosive liquid. Poisonous liquid. Stop leak if without risk. Absorb with DRY

earth, sand or other non-combustible material. Do not get water inside container.

Do not touch spilled material. Use water spray curtain to divert vapor drift. Use

water spray to reduce vapors. Prevent entry into sewers, basements or confined

areas; dike if needed. Call for assistance on disposal. Neutralize the residue with a

dilute solution of acetic acid. Be careful that the product is not present at a

concentration level above TLV. Check TLV on the MSDS and with local

authorities.

Section 7: Handling and Storage

Precautions:

Keep locked up.. Keep container dry. Do not ingest. Do not breathe gas/fumes/

vapor/spray. Never add water to this product. In case of insufficient ventilation,

wear suitable respiratory equipment. If ingested, seek medical advice immediately

and show the container or the label. Avoid contact with skin and eyes. Keep away

from incompatibles such as metals, acids.

Storage:

Keep container tightly closed. Keep container in a cool, well-ventilated area. Do

not store above 25°C (77°F).

Section 8: Exposure Controls/Personal Protection

Engineering Controls:

Provide exhaust ventilation or other engineering controls to keep the airborne

concentrations of vapors below their respective threshold limit value. Ensure that

eyewash stations and safety showers are proximal to the work-station location.

Personal Protection:

Face shield. Full suit. Vapor respirator. Be sure to use an approved/certified

respirator or equivalent. Gloves. Boots.

Personal Protection in Case of a Large Spill:

Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained

breathing apparatus should be used to avoid inhalation of the product. Suggested

protective clothing might not be sufficient; consult a specialist BEFORE handling

this product.

Section 9: Physical and Chemical Properties

Physical state and appearance: Liquid.

Odor: Ammonia-like (Strong.)

Taste: Acrid.

Molecular Weight: 35.05

Color: Colorless.

pH (1% soln/water): 11.6 [Basic.] This is the actual pH in a 1 N solution.

Melting Point: -69.2°C (-92.6°F)

Specific Gravity: 0.898 (Water = 1)

Vapor Pressure: 287.9 kPa (@ 20°C)

Odor Threshold: 5 - 50 ppm as ammonia

Dispersion Properties: See solubility in water

Solubility: Easily soluble in cold water.

Section 10: Stability and Reactivity Data

Stability: The product is stable.

Conditions of Instability: Incompatible materials, high temperatures

Incompatibility with various substances:

Highly reactive with metals. Reactive with acids. Slightly reactive to reactive with

oxidizing agents.

Corrosivity:

Extremely corrosive in presence of zinc, of copper. Corrosive in presence of

aluminum. Non-corrosive in presence of glass, of stainless steel(304), of stainless

steel(316).

Special Remarks on Reactivity:

Incompatible with the following: Organic acids, amides, organic anhydrides,

isocyanates, vinyl acetate, epichlorhydrin, aldehydes, Acrolein, Acrylic acid,

chlorosulfonic acid, dimethyl sulfate, fluorine, gold + aqua regia, hydrochloric

acid, hydrofluoric acid, hydrogen peroxide, iodine, nitric acid, olelum,

propiolactone, propylene oxide, silver nitrate, silver oxide, silver oxide + ethyl

alcohol, nitromethane, silver permanganate, sulfuric acid, halogens. Forms

explosive compounds with many heavy metals (silver, lead, zinc) and halide salts.

Special Remarks on Corrosivity:

Dissolves copper and zinc. Corrosive to aluminum and its alloys. Corrosive to

galvanized surfaces. Severe corrosive effect on brass and bronze

Polymerization: Will not occur.

Section 11: Toxicological Information

Routes of Entry:

Absorbed through skin. Dermal contact. Eye contact. Inhalation. Ingestion.

Chronic Effects on Humans:

MUTAGENIC EFFECTS: Mutagenic for bacteria and/or yeast. [Ammonium

hydroxide]. May cause damage to the following organs: mucous membranes, skin,

eyes.

Other Toxic Effects on Humans:

Very hazardous in case of skin contact (corrosive, irritant, permeator), of

ingestion, . Hazardous in case of eye contact (corrosive), of inhalation (lung

corrosive).

Special Remarks on Chronic Effects on Humans:

May affect genetic material based on tests with microorganisms and animals. May

cause cancer (tumorigenic) based on animal data. No human data found at this

time. (Ammonia, anhydrous)

Special Remarks on other Toxic Effects on Humans:

Acute Potential Health Effects: Skin: Causes severe irritation. Causes skin burns.

May cause deep, penetrating ulcers of the skin. Contact with skin may cause

staining, inflammation, and thickening of the skin. Eye: Contact with liquid or

vapor causes severe burns and possible irreversible eye damage including corneal

injury and cataracts. Inhalation: Causes severe irritation of the upper respiratory

tract with coughing, burns, breathing difficulty. May cause acute pulmonary

edema, pneumoconiosis, fibrosis, and even coma. It is a respiratory stimulant

when inhaled at lower concentrations. It may also affect behavior/ central nervous

system (convulsions, seizures, ataxia, tremor), cardiovascular system (increase in

blood pressure and pulse rate). Ingestion: Harmful if swallowed. Affects the

Gastrointestinal tract (burns, swelling of the lips, mouth, and larynx, throat

constriction, nausea, vomiting, convulsions, shock, and may cause severe and

permanent damage), liver, and urinary system (kidneys) May affect behavior

(convulsions, seizures, ataxia, excitement).

Chronic Potential Health Effects: Ingestion: May cause effects similar to those of

acute ingestion. Inhalation: Repeated exposure to low concentrations may cause

bronchitis with cough, phlegm, and/or shortness of breath. May also cause liver

and kidney damage, and affect the brain, and blood. Eye: May cause corneal

damage and the development of cataracts and glaucoma. Skin: Repeated skin

contact to low concentrations may cause dryness, itching, and redness (dermatitis)

Protective Equipment:

Gloves. Full suit. Vapor respirator. Be sure to use an approved/certified respirator

or equivalent. Wear appropriate respirator when ventilation is inadequate. Face

shield.

V. TOOLS and MATERIALS :

A. Tools :

Volumetric pipette 25mL

Volumetric flask 250mL

25 % NH3

37,6789 mL NH3 25 %

Take 37,6789 mL by using volumetric pipette in acid roomPoured into volumetric flask 100 mL

Added aquades until reach half apart of volumetric flaskWhile shake it slowly, in order to make it be homogenous mixture (perfectly mixed)

NH4OH solution

Added aquades again until reach sign line in measure flask

250 mL NH4OH 25% diluted

Beaker glass 100mL

Pipette

B. Materials:

NH3 solution

Aquades

VI. FLOWCHART

VII. PROCEDURE

1. Calculating the mass of NH3 which is required to prepare 250 mL of NH4OH 2 M .

Then it is obtained 903 gram for NH3

2. Converting mass of NH3 obtained into concentration. And the concentration obtained

is 13,279 M

3. Calculating the volume of NH3 from the concentration, 13,279 M. Then, finding the

volume of NH3 is 37,6789 mL

4. Pouring NH3 into volumetric flask 37,6789 mL by using volumetric pipette

5. Diluting NH3 by adding aquades half portion of volumetric flask

6. While shaking until the solution be homogenous mixture (perfectly mixed)

7. Adding aquades again into volumetric flask until reach the sign line.

VIII. RESULT AND DISCUSSION :

NH4OH solution is the solution that prepared from NH3 in liquid phase. Where the preparation of solution is diluting solution by adding aquades. In this experiment, the volume needed of NH4OH 2 M is 250 mL. Before preparing the solution of NH4OH . the calculating of concentration and volume must be done. To calculate the concentration, volume of NH3 that required by using this formulation.Known% NH3 = 25%ρ NH3 = 0.903 kg/LAskedV NH3 needed to make NH4OH solution 2M 250 mL?Answer1. Determine the molarity of source solution.2. Determine the V of source solution needed to make NH4OH solution 2M 250 mL

Determining the molarity of source solution.Mass NH3 in 1L (g) = V (mL) x ρ (g/mL) = 1000 x 0.903 = 903 gMass NH3 in NH3 25% (g) = percentage (%) x mass (g)

= 225,75 g

Molarity (M)

= 13.279 M

Determining the Volume of source solution needed

37,6789 mLof NH3 is poured into volumetric flask by using volumetric pipette. And diluted it by adding aquades for half portion initially of volumetric flask. And shaking for while time , in order to make the solution be homogenous mixture.

After the solution perfectly mixed, adding aquades into that mixture until reach the sign line (250 mL). Finally, 250 mL of 25 % NH4OH 2 M solution have already prepared. And the color of solution is colorless. And then labeling the solution on the volumetric flask.

IX. CONCLUSION :

Preparation 250 mL of 25% NH4OH 2M is needed NH3 37,6789 mL. And it is also accompanied with diluting process.

ATTACHMENT PICTURE

REFFERNCES

Grow HOW. 2008. Material Safety Data Sheet Amonia Solution. (Online) http://www.growhow.co.uk/documents/chemicalproducts_psds/ammonia_solution_msds13aug08.pdf. Accessed on 05 March 2014 at 10.23 WIB

Mitarlis, Utiya Azizah, dan Amaria. 2010. Organisasi dan Manajemen Laboratorium Pendidikan Kimia. Surabaya: UNESA University Prees.

Puspita, Fika. 2013. Laporan Pembuatan Larutan. (Online) http://fikapuspita.blogspot.com/2013/07/laporan-pembuatan-larutan_9195.html. Accessed on 06 March 2014 at 11.47 WIB

Figure 1. Taking solution of NH3 in acid room

Figure 2. poured solution in volumetric flask

Figure 4. NH4OH solution have been prepared by adding aquadest again until reach the sign line